CN107880316A - A kind of preparation method of the anti-molten drop fire retardant of thermostabilization - Google Patents

A kind of preparation method of the anti-molten drop fire retardant of thermostabilization Download PDF

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CN107880316A
CN107880316A CN201711083289.8A CN201711083289A CN107880316A CN 107880316 A CN107880316 A CN 107880316A CN 201711083289 A CN201711083289 A CN 201711083289A CN 107880316 A CN107880316 A CN 107880316A
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fire retardant
graphite
added
molten drop
temperature
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周德峰
何俊欣
陈莉莉
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Changzhou LAN Sen environmental protection equipment Co., Ltd.
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Changzhou Fulong Industrial Equipment Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of preparation method of the anti-molten drop fire retardant of thermostabilization, belong to technical field of flame retardant agent preparation.With polyurethane polyurethane micro-encapsulated expansiveness graphite is made in expansiveness graphite coat by the present invention,Silica hydrogel microencapsulation APP is made with Silica hydrogel coated ammonium polyphosphate,Two kinds of products of gained are blended in cellulose gel,Dry,Melting pelletizing obtains the anti-molten drop fire retardant of thermostabilization,Reach fire-retardant purpose,Expansible graphite is that natural flake graphite passes through a series of oxidation intercalations,In graphite flake Intercalation reaction nitric acid,The compounds such as sulfuric acid,And the graphite with interlayer intercalation thing formed,Under the high temperature conditions,Intercalator is heated rapid vaporization,The gas of formation will produce to graphite flake layer huge supports power,And the lamella expansion made,Form the adiabatic layer of charcoal of densification,Even if high temperature is with the presence of polymer molten drop,The defects of so as to improve polyurethane foam plastics melting drippage,This above has a extensive future in communal facility application.

Description

A kind of preparation method of the anti-molten drop fire retardant of thermostabilization
Technical field
The invention discloses a kind of preparation method of the anti-molten drop fire retardant of thermostabilization, belong to technical field of flame retardant agent preparation.
Background technology
Fire retardant, assigns the functional aid of combustible polymers flame retardancy, and fire-retardant primarily directed to high polymer material sets Meter;Fire retardant has polytype, is divided into additive flame retardant and reactive flame retardant by application method.
Additive flame retardant is to be added to by mechanical mix techniques in polymer, polymer is had anti-flammability, mesh Preceding additive flame retardant mainly has organic fire-retardant and inorganic combustion inhibitor, halogenated flame retardant and non-halogen.Organic is with bromine system, phosphorus nitrogen System, nitrogen system and red phosphorus and some fire retardants that compound is representative, inorganic mainly antimony oxide, magnesium hydroxide, hydroxide The flame-retardant systems such as aluminium, silicon systems.
For the material of high polymer material flame resistance can be increased, it is mainly used in high polymer material such as plastics, rubber, fiber Deng, and most of these materials can burn.Particularly plastics, applied in communications and transportation, building, electricity Gong Qi Material, aviation, space flight etc., it is felt to be desirable to solve its resistance to combustion problem.The use of fire retardant should typically possess following Several conditions:The physical property of high polymer material is not reduced, such as heat resistance, mechanical strength, electric property;Decomposition temperature should not be too high, But it can not decompose again at processing temperatures;Good endurance;Good weatherability.
Fire-retardant science and technology is to adapt to the needs of social safety production and life, and fire preventing occurs, and protects the people Lives and properties and a science to grow up.Fire retardant is application of the flame-retarded technology in real life, and it is that one kind is used for Improve the special auxiliary chemicals of flammable combustible material combustibility, be widely used in the fire-retardant processing of all kinds of finishing materials. Material after fire retardant is processed, when being attacked by extraneous burning things which may cause a fire disaster, it can effectively prevent, delay or terminate the biography of flame Broadcast, it is fire-retardant so as to have the function that.All there is heat endurance difference in the fire retardant largely used at present and polymer is easily high The defects of temperature melting drippage, therefore, invent a kind of anti-molten drop fire retardant of thermostabilization has actively to technical field of flame retardant agent preparation Meaning.
The content of the invention
Present invention mainly solves technical problem, for fire retardant heat endurance difference and polyurethane foam plastics easily in height A kind of the defects of lower melting of temperature is dripped, there is provided preparation method of the anti-molten drop fire retardant of thermostabilization.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of the anti-molten drop fire retardant of thermostabilization, it is characterised in that specifically preparation process is:
(1)Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, add 14~16g pentaerythrites and 200~ 230mL dimethyl sulfoxide (DMSO)s, heat temperature raising, start after agitator stirs to pentaerythrite and be completely dissolved, 35 are added to four-hole boiling flask ~37g Toluene-2,4-diisocyanates, 4- diisocyanate, 200~220mL1,4- dioxane, obtain pre-dispersed material;
(2)200~300g expansible graphites, 3~5gOP-10,250~300 mL1,4- dioxies are added into above-mentioned pre-dispersed material Six rings, reacted after being heated up to above-mentioned four-hole boiling flask, naturally cool to room temperature, obtain reaction product, filtered, removed filtrate and filtered Slag, by filter residue with after distillation water washing, it is put into baking oven, heat temperature raising, dries, obtain polyurethane micro-encapsulated expansiveness stone Ink;
(3)100~120g APPs, 230~250mL absolute ethyl alcohols, 100~200mL distilled water, stirring are added into beaker Mixing, ammoniacal liquor regulation pH is added into beaker, obtains the material that alkalizes, 20~25g methyl triethoxies are added into alkalization material Silane, to beaker water-bath heat temperature raising, insulation reaction, filter off except liquid, obtain gel, after gel is used into distillation water washing, It is put into baking oven, heat temperature raising, dries, obtain Silica hydrogel microencapsulation APP;
(4)Count in parts by weight, 4~6 parts of acetylbutyrylcelluloses, 80~90 parts of ethyl acetate are added with agitator and returned In the three-necked flask for flowing condenser pipe, start agitator, stirring, by 40~50 parts of polyurethane micro-encapsulated expansiveness graphite and 30 ~35 parts of Silica hydrogel microencapsulation APPs are added in three-necked flask, are dispersed with stirring, and obtain mixing disperse materials;
(5)Mixing disperse materials are placed in vacuum drying chamber, is dried, is placed in double screw extruder, pelletizing, obtains fire retardant.
Step(1)Temperature is 40~50 DEG C after described heat temperature raising, and agitator speed is 300~400r/min.
Step(2)The particle diameter of described expansible graphite is 300 mesh, and temperature is 80~85 DEG C after heating, the reaction time 5 ~8h, temperature is 100~105 DEG C after baking oven heat temperature raising, and filter residue distilled water washing times are 3~5 times, drying time 6 ~10h.
Step(3)The described time that is stirred is 20~25min, and the mass fraction of ammoniacal liquor is 35%, adds ammoniacal liquor regulation PH is 10.2~10.4, and temperature is 45~60 DEG C after heating water bath heating, and the insulation reaction time is 2~3h, gel distilled water Washing times are 2~3 times, and temperature is 80~90 DEG C after baking oven heat temperature raising, and drying time is 5~6h.
Step(4)Described agitator speed is 400~450r/min, and it is 30~40min to be dispersed with stirring the time.
Step(5)Described vacuum drying chamber design temperature is 60~70 DEG C, and drying time is 6~7h, controls head temperature Spend for 90~100 DEG C, pelletizing speed is 6~8mm/s.
The beneficial effects of the invention are as follows:
(1)With polyurethane polyurethane micro-encapsulated expansiveness graphite is made in expansiveness graphite coat by the present invention, is coagulated with silicon Silica hydrogel microencapsulation APP is made in glue coated ammonium polyphosphate, and two kinds of products of gained are blended in cellulose gel, be dry Dry, melting pelletizing obtains the anti-molten drop fire retardant of thermostabilization, and element silicon has higher heat in Silica hydrogel microencapsulation APP Stability, stable silicon oxide compound can be produced in high temperature, and silicon oxide compound increases the heat endurance of fire retardant in high temperature Add, microcapsule structure plays starvation effect, makes P elements not oxidized, so as to improve the heat endurance of fire retardant;
(2)When the polyurethane foam plastics containing APP is ignited by high temperature, APP is decomposed and is catalyzed poly- the present invention Dehydration carburizing reagent occurs for urethane, generates coke layer, and coke layer is fire retardant, and there is heat-insulated oxygen barrier to prevent burning, cause thermal conductivity to become Difference, reduce base material heated amount, thermal decomposition rate is slack-off, and APP decomposes to obtain phosphoric acid, aggregates into polyphosphoric acid, and polyphosphoric acid is The non-combustible matter of melten glass shape, the conduction that comburant surface prevents oxygen, fuel gas and heat can be covered in, reaches fire-retardant Purpose, heat in high temperature is set to be difficult to conduction into polyurethane, polyurethane would not melt, and expansible graphite is natural scale Graphite passes through a series of oxidation intercalations, and in compounds such as graphite flake Intercalation reaction nitric acid, sulfuric acid, and what is formed has interlayer The graphite of intercalation thing, under the high temperature conditions, intercalator are heated rapid vaporization, and the gas of formation will produce huge to graphite flake layer Power is supported, and the lamella expansion made, expansion multiple can be up to decades of times to hundreds times or even thousands of times, by original flakey Become the very low vermiform of density, the adiabatic layer of charcoal of densification is formd, even if high temperature can also flow to stone with the presence of polymer molten drop Ink sheet interlayer, the external world will not be dropped onto, so as to improve the defects of polyurethane foam plastics melting is dripped, this should in communal facility Use and have a extensive future.
Embodiment
Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, 14~16g pentaerythrites and 200 are added ~230mL dimethyl sulfoxide (DMSO)s, are heated to 40~50 DEG C, start agitator, with 300~400r/min rotating speed stir to After pentaerythrite is completely dissolved, 35~37g Toluene-2,4-diisocyanates, 4- diisocyanate, 200~220mL1,4- bis- are added to four-hole boiling flask The ring of oxygen six, obtains pre-dispersed material;Add the expansible graphite that 200~300g particle diameters are 300 mesh into above-mentioned pre-dispersed material, 3~ 5gOP-10,250~300 mL1,4- dioxane, 80~85 DEG C are warming up to above-mentioned four-hole boiling flask, react 5~8h, it is naturally cold But to room temperature, reaction product is obtained, is filtered, filtrate is removed and obtains filter residue, by filter residue with after distillation water washing 3~5 times, is put into baking In case, 100~105 DEG C are heated to, 6~10h is dried, obtains polyurethane micro-encapsulated expansiveness graphite;Into beaker 100~120g APPs, 230~250mL absolute ethyl alcohols, 100~200mL distilled water are added, is stirred 20~25min, It is 10.2~10.4 that the ammoniacal liquor regulation pH that mass fraction is 35% is added into beaker, obtains the material that alkalizes, adds into alkalization material Enter 20~25g MTESs, 45~60 DEG C are heated to beaker water-bath, 2~3h of insulation reaction, is filtered off Except liquid, gel is obtained, by gel with after distillation water washing 2~3 times, is put into baking oven, is heated to 80~90 DEG C, dry 5~6h, obtain Silica hydrogel microencapsulation APP;Count in parts by weight, by 4~6 parts of acetylbutyrylcelluloses, 80~90 parts Ethyl acetate is added in the three-necked flask with agitator and reflux condensing tube, starts agitator, with turning for 400~450r/min Speed starts to stir, by 40~50 parts of polyurethane micro-encapsulated expansiveness graphite and 30~35 parts of Silica hydrogel microencapsulation polyphosphoric acids Ammonium is added in three-necked flask, is dispersed with stirring 30~40min, obtains mixing disperse materials;Mixing disperse materials are placed in into design temperature is In 60~70 DEG C of vacuum drying chamber, 6~7h is dried, is placed in double screw extruder, it is 90~100 DEG C to control head temperature, Pelletizing is carried out with 6~8mm/s speed, obtains fire retardant.
Example 1
Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, 14g pentaerythrites and 200mL dimethyl are added Sulfoxide, 40 DEG C are heated to, start agitator, stirred with 300r/min rotating speed to pentaerythrite after being completely dissolved, Xiang Si Mouth flask adds 35g Toluene-2,4-diisocyanates, 4- diisocyanate, 200mL1,4- dioxane, obtains pre-dispersed material;To above-mentioned pre-dispersed The expansible graphite that 200g particle diameters are 300 mesh, 3gOP-10,250mL1,4- dioxane, to above-mentioned four-hole boiling flask are added in material 80 DEG C are warming up to, 5h is reacted, naturally cools to room temperature, obtain reaction product, is filtered, filtrate is removed and obtains filter residue, filter residue is used After distillation water washing 3 times, it is put into baking oven, is heated to 100 DEG C, dries 6h, obtain polyurethane micro-encapsulated expansiveness Graphite;100g APPs, 230mL absolute ethyl alcohols, 100mL distilled water are added into beaker, 20min is stirred, to beaker The ammoniacal liquor regulation pH that middle addition mass fraction is 35% is 10.2, obtains the material that alkalizes, 20g methyl three is added into alkalization material Ethoxysilane, 45 DEG C are heated to beaker water-bath, insulation reaction 2h, filters off except liquid, obtains gel, gel is used After distillation water washing 2 times, it is put into baking oven, is heated to 80 DEG C, dries 5h, obtain Silica hydrogel microencapsulation APP; Count in parts by weight, 4 parts of acetylbutyrylcelluloses, 80 parts of ethyl acetate are added to three mouthfuls with agitator and reflux condensing tube In flask, start agitator, start to stir with 400r/min rotating speed, by 40 parts of polyurethane micro-encapsulated expansiveness graphite and 30 parts of Silica hydrogel microencapsulation APPs are added in three-necked flask, are dispersed with stirring 30min, obtain mixing disperse materials;Will mixing Disperse materials are placed in the vacuum drying chamber that design temperature is 60 DEG C, are dried 6h, are placed in double screw extruder, control head temperature For 90 DEG C, pelletizing is carried out with 6mm/s speed, obtains fire retardant.
Example 2
Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, 15g pentaerythrites and 215mL dimethyl are added Sulfoxide, 45 DEG C are heated to, start agitator, stirred with 350r/min rotating speed to pentaerythrite after being completely dissolved, Xiang Si Mouth flask adds 36g Toluene-2,4-diisocyanates, 4- diisocyanate, 210mL1,4- dioxane, obtains pre-dispersed material;To above-mentioned pre-dispersed The expansible graphite that 200~300g particle diameters are 300 mesh, 4gOP-10,270 mL1,4- dioxane, to above-mentioned four are added in material Mouth flask is warming up to 82 DEG C, reacts 6h, naturally cools to room temperature, obtain reaction product, filters, and removes filtrate and obtains filter residue, will Filter residue is put into baking oven with after distillation water washing 4 times, is heated to 102 DEG C, dried 8h, obtain it is polyurethane micro-encapsulated can Expansile graphite;110g APPs, 240mL absolute ethyl alcohols, 150mL distilled water are added into beaker, is stirred 22min, It is 10.3 that the ammoniacal liquor regulation pH that mass fraction is 35% is added into beaker, obtains the material that alkalizes, 22g is added into alkalization material MTESs, 55 DEG C are heated to beaker water-bath, insulation reaction 2.5h, filters off except liquid, obtains gel, By gel with after distillation water washing 2 times, it is put into baking oven, is heated to 85 DEG C, dry 5.5h, obtain Silica hydrogel microencapsulation APP;Count in parts by weight, 5 parts of acetylbutyrylcelluloses, 85 parts of ethyl acetate are added and carry agitator and returned cold In the three-necked flask of solidifying pipe, start agitator, start to stir with 425r/min rotating speed, by 45 parts it is polyurethane micro-encapsulated can be swollen Swollen property graphite and 32 parts of Silica hydrogel microencapsulation APPs are added in three-necked flask, are dispersed with stirring 35min, it is scattered to obtain mixing Material;Disperse materials will be mixed to be placed in the vacuum drying chamber that design temperature is 65 DEG C, 6.5h is dried, be placed in double screw extruder, It is 95 DEG C to control head temperature, carries out pelletizing with 7mm/s speed, obtains fire retardant.
Example 3
Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, 16g pentaerythrites and 230mL dimethyl are added Sulfoxide, 50 DEG C are heated to, start agitator, stirred with 400r/min rotating speed to pentaerythrite after being completely dissolved, Xiang Si Mouth flask adds 37g Toluene-2,4-diisocyanates, 4- diisocyanate, 220mL1,4- dioxane, obtains pre-dispersed material;To above-mentioned pre-dispersed The expansible graphite that 300g particle diameters are 300 mesh is added in material, 5gOP-10,300 mL1,4- dioxane, above-mentioned four mouthfuls are burnt Bottle is warming up to 85 DEG C, reacts 8h, naturally cools to room temperature, obtain reaction product, filters, and removes filtrate and obtains filter residue, by filter residue After distillation water washing 5 times, it is put into baking oven, is heated to 105 DEG C, dry 10h, obtains polyurethane micro-encapsulated inflatable Property graphite;120g APPs, 250mL absolute ethyl alcohols, 200mL distilled water are added into beaker, 25min is stirred, to burning It is 10.4 that the ammoniacal liquor regulation pH that mass fraction is 35% is added in cup, obtains the material that alkalizes, 25g methyl is added into alkalization material Triethoxysilane, 60 DEG C are heated to beaker water-bath, insulation reaction 3h, filters off except liquid, obtains gel, by gel After distillation water washing 3 times, it is put into baking oven, is heated to 90 DEG C, dries 6h, obtain Silica hydrogel microencapsulation polyphosphoric acid Ammonium;Count in parts by weight, 6 parts of acetylbutyrylcelluloses, 90 parts of ethyl acetate are added with agitator and reflux condensing tube In three-necked flask, start agitator, start to stir with 450r/min rotating speed, by 50 parts of polyurethane micro-encapsulated expansiveness stones Ink and 35 parts of Silica hydrogel microencapsulation APPs are added in three-necked flask, are dispersed with stirring 40min, obtain mixing disperse materials;Will Mixing disperse materials are placed in the vacuum drying chamber that design temperature is 70 DEG C, are dried 7h, are placed in double screw extruder, control head Temperature is 100 DEG C, carries out pelletizing with 8mm/s speed, obtains fire retardant.
Comparative example
With the anti-molten drop fire retardant of thermostabilization of Hebei company production as a comparison case to the anti-molten drop of thermostabilization produced by the present invention The anti-molten drop fire retardant of thermostabilization in fire retardant and comparative example carries out performance detection, and testing result is as shown in table 1:
1st, method of testing:
High-temperature fusion drips method of testing:It is standby to prepare isocyanates, polyethers, foaming agent, the catalyst of four parts of equivalent, takes equivalent Example 1~3 and fire retardant in comparative example and isocyanates, polyethers, foaming agent, catalyst mixed by special equipment, pass through The high molecular polymer that high pressure painting foam-in-place forms, then the high molecular polymer that foaming is formed are put into baking oven, are modulated Temperature is 500 DEG C, observes its drippage situation;
Table 1
Test event Example 1 Example 2 Example 3 Comparative example
Drippage situation Situation without dripping off Situation without dripping off Situation without dripping off Obvious drippage
Decomposition temperature(℃) 512 518 520 455
It can be seen from above-mentioned middle data, the drippage situation of the anti-molten drop fire retardant of thermostabilization produced by the present invention is excellent, in high tender feeling Under condition, there is not molten drop phenomenon, decomposition temperature is both greater than 480 DEG C so that remaining carbon is high, forms relatively stable carbon-coating, makes Obtain material and show preferable heat endurance in the case where being further heated, therefore, the anti-molten drop of thermostabilization produced by the present invention Fire retardant has broad application prospects.

Claims (6)

1. a kind of preparation method of the anti-molten drop fire retardant of thermostabilization, it is characterised in that specifically preparation process is:
(1)Into the four-hole boiling flask with thermometer, agitator and reflux condensing tube, add 14~16g pentaerythrites and 200~ 230mL dimethyl sulfoxide (DMSO)s, heat temperature raising, start after agitator stirs to pentaerythrite and be completely dissolved, 35 are added to four-hole boiling flask ~37g Toluene-2,4-diisocyanates, 4- diisocyanate, 200~220mL1,4- dioxane, obtain pre-dispersed material;
(2)200~300g expansible graphites, 3~5gOP-10,250~300 mL1,4- dioxies are added into above-mentioned pre-dispersed material Six rings, reacted after being heated up to above-mentioned four-hole boiling flask, naturally cool to room temperature, obtain reaction product, filtered, removed filtrate and filtered Slag, by filter residue with after distillation water washing, it is put into baking oven, heat temperature raising, dries, obtain polyurethane micro-encapsulated expansiveness stone Ink;
(3)100~120g APPs, 230~250mL absolute ethyl alcohols, 100~200mL distilled water, stirring are added into beaker Mixing, ammoniacal liquor regulation pH is added into beaker, obtains the material that alkalizes, 20~25g methyl triethoxies are added into alkalization material Silane, to beaker water-bath heat temperature raising, insulation reaction, filter off except liquid, obtain gel, after gel is used into distillation water washing, It is put into baking oven, heat temperature raising, dries, obtain Silica hydrogel microencapsulation APP;
(4)Count in parts by weight, 4~6 parts of acetylbutyrylcelluloses, 80~90 parts of ethyl acetate are added with agitator and returned In the three-necked flask for flowing condenser pipe, start agitator, stirring, by 40~50 parts of polyurethane micro-encapsulated expansiveness graphite and 30 ~35 parts of Silica hydrogel microencapsulation APPs are added in three-necked flask, are dispersed with stirring, and obtain mixing disperse materials;
(5)Mixing disperse materials are placed in vacuum drying chamber, is dried, is placed in double screw extruder, pelletizing, obtains fire retardant.
A kind of 2. preparation method of the anti-molten drop fire retardant of thermostabilization according to claim 1, it is characterised in that:Step(1) Temperature is 40~50 DEG C after described heat temperature raising, and agitator speed is 300~400r/min.
A kind of 3. preparation method of the anti-molten drop fire retardant of thermostabilization according to claim 1, it is characterised in that:Step(2) The particle diameter of described expansible graphite is 300 mesh, and temperature is 80~85 DEG C after heating, and the reaction time is 5~8h, and baking oven heating rises Temperature is 100~105 DEG C after temperature, and filter residue distilled water washing times are 3~5 times, and drying time is 6~10h.
A kind of 4. preparation method of the anti-molten drop fire retardant of thermostabilization according to claim 1, it is characterised in that:Step(3) The described time that is stirred is 20~25min, and the mass fraction of ammoniacal liquor is 35%, and it is 10.2~10.4 to add ammoniacal liquor regulation pH, Temperature is 45~60 DEG C after heating water bath heating, and the insulation reaction time is 2~3h, and gel distilled water washing times are 2~3 Secondary, temperature is 80~90 DEG C after baking oven heat temperature raising, and drying time is 5~6h.
A kind of 5. preparation method of the anti-molten drop fire retardant of thermostabilization according to claim 1, it is characterised in that:Step(4) Described agitator speed is 400~450r/min, and it is 30~40min to be dispersed with stirring the time.
A kind of 6. preparation method of the anti-molten drop fire retardant of thermostabilization according to claim 1, it is characterised in that:Step(5) Described vacuum drying chamber design temperature is 60~70 DEG C, and drying time is 6~7h, and it is 90~100 DEG C to control head temperature, is cut Grain speed is 6~8mm/s.
CN201711083289.8A 2017-11-07 2017-11-07 A kind of preparation method of the anti-molten drop fire retardant of thermostabilization Pending CN107880316A (en)

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CN108504285A (en) * 2018-04-09 2018-09-07 徐冬 A kind of preparation method of food packaging fire-retardant bubble chamber film
CN110592709A (en) * 2019-09-11 2019-12-20 东华大学 Preparation method of flame-retardant anti-dripping polyester fiber
CN110713767A (en) * 2019-11-14 2020-01-21 福建南烽防火科技有限公司 Green intumescent home decoration fireproof water paint and preparation method thereof
CN113549310A (en) * 2021-08-12 2021-10-26 福州大学 Low-smoke flame-retardant polylactic acid composite material and preparation method thereof
CN115490922A (en) * 2022-11-16 2022-12-20 鲁东大学 Polyurethane-coated expandable graphite flame retardant and preparation method thereof

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CN105925168A (en) * 2016-05-20 2016-09-07 武汉工程大学 Microencapsulated water-based fire retardant coating and preparation method thereof

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